Acetonitrile → 72821-03-5

HRID 1706678Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1706678
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.I[CH2:10][Si:11]([CH3:19])([CH3:18])[O:12][Si:13]([CH2:16]I)([CH3:15])[CH3:14].C(#N)C.CCCCC>O>[CH2:1]([N:8]1[CH2:14][Si:13]([CH3:16])([CH3:15])[O:12][Si:11]([CH3:19])([CH3:18])[CH2:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 6342AcetonitrileHCID 7504BenzylamineHCID 8003PentaneHCID 2566811,3-Bis(iodomethyl)-1,1,3,3-tetramethyldisiloxane

Produkt 1

HCID 2033392972821-03-5

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

An amount of 33.6 g. (0.315 mole) of benzylamine is added over a period of approximately 5 minutes to 41.4 g. (0.1 mole) of 1,3-bis-iodomethyl-1,1,3,3-tetramethyl-disiloxane with stirring in a bath at room temperature. Stirring is continued at room temperature for one hour. (A slurry resulted). Addition of 50 ml. of acetonitrile gives a clear solution which is then heated to reflux for 2 hours. The cooled solution is distributed between approximately 0.5 l. of pentane and 1.5 l. of water. The aqueous layer is then extracted with one more approximately 200 ml. portion of pentane, and the combined organic layer is washed twice with approximately 300 ml. of water, dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to provide a clear yellow mobile liquid. This product is then vacuum distilled to give 4-benzyl-2,2,6,6-tetramethyl-1-oxa-4-aza-2,6-disilacyclohexane; b.p. 134° to 135° C., at 13 mm Hg.

Aufarbeitung

  1. custom(A slurry resulted)
  2. additionAddition of 50 ml
  3. temperatureis then heated
  4. temperatureto reflux for 2 hours
  5. extractionThe aqueous layer is then extracted with one more approximately 200 ml
  6. washportion of pentane, and the combined organic layer is washed twice with approximately 300 ml
  7. dry with materialof water, dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customevaporated in vacuo
  10. customto provide a clear yellow mobile liquid
  11. distillationvacuum distilled

Quellen und Nachweise

ORD-Eintrag
ord-1590b6c79e544e76948a513e2650e065
Quelldatensatz
uspto-grants-1980_06
Patentnummer
US04208408

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